Process for treating textile materials

ABSTRACT

A process and an apparatus for batch treating of textile material such as yarn packages, raw stock, knit goods, muffs or the like by placing the material in an enclosed zone, evacuating the enclosed zone to provide a vacuum therein, and then flooding the evacuated zone with a treating agent by placing the evacuated zone into communication with a second zone having the treating agent therein under a positive pressure. A substantial pressure differential exists between the two zones, and the treating agent flows extremely rapidly through the textile material whereby, at the very outset of the treating process, the treating agent is uniformly distributed over the surfaces of the textile material and substantially in its original concentration and condition. The temperature of the treating agent will depend upon the treatment. The process and apparatus are capable of recycling or reversing the flow of the treating agent through the textile material as and when desired. Examples of treating agents are: dye liquor, scouring liquids, fixing agents, solvents, finishes or the like, or combinations of dye liquor with other treating agents, such as scouring chemicals, salt, and any other desired chemicals.

nited States Patent [191 Wedler 1 Nov. 27, 1973 [22] Filed:

[ 1 PROCESS FOR TREATING TEXTILE MATERIALS 7 [75] lnventor: Frederick C.Wedler, Greensboro,

[73] Assignee: Burlington Industries, Inc.,

Greensboro, NC.

Jan. 25, 1971 [21] Appl. No.: 109,501

Related US. Application Data [63] Continuation-impart of Ser. No.746,973, July 23,

1968, abandoned.

[52] US. Cl. 8/l55.1 [51] Int. Cl. B05c 8/02 [58] Field of Search8/149.1, 149.2, 149.3,

Primary Examiner-William 1. Price Attorney-Cushman, Darby & Cushman 5 7]ABSTRACT A process and an apparatus for batch treating of textilematerial such as yarn packages, raw stock, knit goods, muffs or the likeby placing the material in an enclosed zone, evacuating the enclosedzone to provide a vacuum therein, and then flooding the evacuated zonewith a treating agent by placing the evacuated zone into communicationwith a second zone having the treating agent therein under a positivepressure. A substantial pressure differential exists between the twozones, and the treating agent flows extremely rapidly through thetextile material whereby, at the very outset of the treating process,the treating agent is uniformly distributed over the surfaces of thetextile material and substantially in its original concentration andcondition.

The temperature of the treating agent will depend upon the treatment.The process and apparatus are capable of recycling or reversing the flowof the treating agent through the textile material as and when desired.Examples of treating agents are: dye liquor, scouring liquids, fixingagents, solvents, finishes or the like, or combinations of dye liquorwith other treating agents, such as scouring chemicals, salt, and anyother desired chemicals.

24 Claims, 4 Drawing Figures United States Patent [1 1 [1 1 3,775,055Wedler Nov. 27, 1973 PATENTEDNBY 21 ms lv vw gm in H INVENTOR FFMDHP/C/rC M5015? ATTORNEYS 68 wwwu zqw PROCESS FOR TREATING TEXTILE MATERIALSThis application is a continuation-in-part of my copending application,Ser. No. 746,973, filed July 23, 1968 now abandoned.

The present invention is concerned with improved process techniques andapparatus for batch treatment of textile materials such as yarnpackages, raw stock, fabrics, or other forms of textile materials in anappropriate sequence of vacuum conditions and with fluid treating agentssuch as dye liquor, scouring liquids, fixing agents, solvents, finishes,or the like, or combinations of dye liquor with other treating agents,such as scouring chemicals, salt, and any other desired chemicals.

While the invention is capable of use in the batch treatment of varioustypes of textile materials the invention will be illustrated anddiscussed with particular reference to the dyeing of yarn packages andrelated processing.

in forming yarn packages in the textile industry, yarn is commonlyuniformly wound on perforated spools, tubes or springs or it is commonlywound to form a package on appropriate textile winding equipment, thepackage being removed from that equipment so as to have an open boretherethrough.

A serious problem encountered in connection with conventional processesfor dyeing such yarn packages is that of exhaustion. An importantexample of this problem relates to the early stages of dyeing, and inconventional processes, the layer of yarn first contacted by the dyewill be most heavily dyed, and the liquor will become progressively lessconcentrated as it moves through subsequent layers of yarn, yielding ortending to yield uneven or poor levelness in the dyed yarn. The amountof dye absorbed in the first few seconds of dyeing known technically asthe strike of the dye has been recognized to be of the utmostimportance.

The present invention recognizes the importance of these first fewseconds of the dyeing process and it provides a novel method andapparatus whereby dye solution is uniformly distributed substantiallyinstantaneously over the surfaces of the textile material to be dyed,and at the very outset of the dyeing process. It will be appreciatedthat the broad concept of the present invention may be applied withgreat advantage to fluid treating processes, other than dyeing, fortextile materials, although it has been found to produce outstanding,unexpected and superior results in dyeing processes. Not only does ityield a final product with desirable color uniformity throughout, but itsignificantly shortens processing times.

Broadly stated, the present process involves placing the textilematerial, for example, the yarn package or packages, in an enclosedzone, the zone then being evacuated so as to place the package under apredetermined and substantial vacuum. By subjecting the package to betreated to a high vacuum or high negative pressure in an enclosed zone,the package is desirably degassed so that as much air, vapor and gassesas is practicable are removed from the yarn prior to processing. Asecond zone having the treating agent therein may be suitably heated toa predetermined temperature as determined by the process. the secondzone is under a higher pressure than exists in the vacuum zone, forexample, a positive superatmospheric pressure.

The two zones are then suddenly placed in communication, and due to thegreat pressure differential between the two zones and the conduit andvalve means used, the treating agent from the second zone flowsextremely rapidly into the low pressure zone, flowing through thepackage or packages, in exemplary embodiments, from the interior to theexterior thereof. This extremely rapid flow results in the surfaces ofthe textile material being exposed to the treating agent substantiallyinstantaneously, or within a few seconds. Thus, the concentration andcondition of the treating agent is substantially the same during itspassage through the entire yarn package as it is at the very outset ofthe treating process.

The application of the broad concept of the present invention todifferent types of processing operations, for example dyeing, fordifferent types of textile material has led to further improvements, aswill become evident.

Foreign materials on the surface of or within the yarns or fabricspresented for dyeing have always been a problem due to their tendency tocause uneven application of the dye resulting in poor levelness of thedyed yarn. These foreign materials are normally spin finish, dirt pickedup during prior processing, spinning lubricants, coning oils, naturalwaxes, sizings, and natural contaminants which are particularly presenton cotton and wool. Good dyeing practice has always dictated the removalof these foreign substances by a pre-scour by scouring chemicals such assoda ash, other alkaline materials, wetting agents and other scouringassistants. Pre-scour is normally carried out under heat and pressure.The time necessary to raise the temperature to desired levels and carryout the scouring is normally 45-60 minutes. This process has been a slowone because the textiles being treated are hydrophobic in nature andtend to resist wetting by water and waterborne chemicals.

Therefore, it has been necessary in the past to use special wettingagents, complexing agents, and other systems, as well as heat andpressure, in order to bring about contaminant removal. Thus, it wouldnot normally occur to one skilled in the art of dyeing to mix thescouring chemicals with the dye bath in order to simultaneously scourand dye in the same bath. However, this idea developed out of observingthe pronounced increase in wetting and penetration of yarn brought aboutby the removal of the occluded air, gasses and vapors due to the vacuumstep of the present invention.

The process of the invention including vacuum removal of occluded air,gasses and vapors has so enhanced the wetting and penetration of yarn,that it has been found possible by the methods set forth hereinbelow tosimultaneously scour and dye yarn in the same bath in a number of typesof dyeing operations. These types of dyeing include, for example, directdyeing on cellulosic fibers and yarns, dispersed dyeing of yarns andknitted fabrics, naphthol dyeing of cellulosic fibers and vat dyeing ofcellulosic fibers. It has also been found that the separate pre-scourstep normally involved in dyeing processes for wool and polyester/woolblended yarns may be eliminated.

Other objects and advantages of the present invention will becomeapparent from the following detailed description which refers, in part,to the accompanying drawings wherein:

FIG. 1 is a diagrammatic vertical sectional view of an exemplaryapparatus for treating a tubewound yarn package with a treating agent,according to the invention,

FIG. 2 is a diagrammatic vertical sectional view corresponding to FIG. 1and showing an alternative manner of connecting certain piping orconduits to the chambers FIG. 3 is an enlarged and diagrammaticfragmentary sectional view of the apparatus of FIG. 1 modified fortreatment of a rocket-wound package, and

FIG. 4 is a fragmentary and reduced, partially sectioned view of amodification of part of the apparatus shown in FIGS. 1, 2, and 3.

Referring to the drawings wherein like character or reference numeralsrepresent like or similar parts, a first tank or kier is generallydesignated at 10 in FIG. 1 and serves to define a vacuum or degassingzone. While the tank or chamber 10 is illustrated as supporting a singletube-wound package TP for the purpose of simplicity in this description,it will be appreciated that the tank or kier 10 may be of conventionalconstruction designed to receive a number of packages TP, if so desired,as will be understood. The tank or chamber 10 is made from sufficientlyrigid material to be able to withstand a strong vacuum, for example, inthe order of 28 inches of mercury (i.e. 2 inches of mercury absolutepressure) or weaker and/or stronger vacuums. Stainless steel or othersuitable material may be used for the tank 10. Tank 10, for the purposeof this description, is provided with a removable cover or lid 12 boltedinto position by bolt means 14 when the package T? is positionedtherein.

A second tank or chamber generally designated at 16, which defines asecond zone for treating agent D, for example dye liquor, scouringliquids, fixing agents, solvents, finishes, or the like, is positionedpreferably above the tank 10 although it may be positioned beside orbelow tank 10. The tank or chamber 16 must be of sufficient volume tocarry a supply of treating agent D capable of flooding any size of tank10 utilized in the system. It will be appreciated that the size of tank10 is dependent upon the number and types of yarn packages TP to betreated. Tank or chamber 16, like tank 10, is made of a rigid materialsuch as stainless steel or other suitable materials, capable ofwithstanding pressures in the order of 50l00 p.s.i. or greater. (As usedherein, p.s.i." or pounds per square inch will mean gauge pressure,unless otherwise indicated.)

Heating means 18 including, for example, a steam generator 20 and closedsteam coils 22 positioned within the tank 16 and immediately above thebottom thereof is provided for heating the treating agent D within thetank to a predetermined desired temperature, the steam generator beingcapable of raising the temperature of the treating agent to 300F, ifdesired. A temperature gauge 24 is provided on the tank 16 for measuringthe temperature of the treating agent D therein.

The tank 16 is provided with an inlet 26 for a conduit 28, the inletbeing utilized either to apply pressure and- /or temperature to tank 16or to apply steam to the interior of the tank. A branch conduit 30leading to a high pressure source of air 32, such as an air compressoror the like, communicates with the conduit 28 by a selectively operablevalve means 34. A pressure gage G mounted on the dome of the tank 16provides visual indication of pressure buildup in the tank 16. A steamgenerator 36 also communicates with the conduit 28 by means of a branchconduit 38 having a selectively operable valve means 40 therein.

Referring back to the tank or kier 10, it will be noted that the yarnpackage TP is a tube-wound package in which the center portion of thetube supporting the windings of yarn is perforated as indicated at 42.In some instances, the tube for the package is merely a rigid tube withholes whereas it could also be either a spring tube or a screen tube thelatter being illustrated in FIG. 1 through which a liquid or vapor caneasily pass. The ends of the tube of the package TP are shown as fittingrespectively into an open collar 44 in the cover 12 and a closed endcollar 46 provided on the bottom 48 of the tank 10. Any suitable sealingmeans 50 may be provided between the respective collars and the tubeends.

A relatively large diameter transfer conduit 52 is shown as beingprovided between the bottom of the tank 16 and the top of the tank 14,there also being provided sealing means 54 between the conduit and thecollar 44. The conduit 52 is provided with a quickopening large volumeselectively operable valve means 56 so that the two tanks 10 and 16 maybe quickly placed into and out of communication with each other.

A source of supply or reservoir for treating agent D is generallyindicated at 58, the source of supply being in communication with aninlet 60 of a conventional high capacity, reversible pump 62. In moredetail, a conduit 64 having a selectively operable valve means 66therein communicates with a conduit 68 also having a selectivelyoperable valve means 70 therein. The conduit 68 also communicates withthe bottom of the tank 10 by means of an outlet conduit 72 having aselectively operable valve means 74 therein.

Since the conduit 52 communicates with the interior of the tube 42, theflow of the treating agent D is from the interior to the exterior of thepackage, as will be evident.

An outlet 76 for pump 62 communicates with the tank 16 by means of aconduit 78, the conduit 78 having selectively operable valve means 80therein, and an outlet 81 open to the interior of tank 16. Outlet 81 isshown in FIG. 1 disposed adjacent the top of the tank 16 but itsposition therein may be varied, as desired. For example, it may bearranged near the bottom of tank 16, below the liquid level, asindicated by numeral 81 in FIG. 2, or it may be disposed at someintermediate point, as will be understood.

In order to evacuate the tank or chamber 10, a high capacity vacuum pump82 is provided and connected to the tank by means of a conduit 84 havinga valve 85 therein, as shown. Conduit 84 may enter tank 10 adjacent thebottom thereof, as shown in FIG. 1, or adjacent the top, as indicated bynumeral 84" in FIG. 2. The vacuum pump 82 withdraws the atmosphere fromwithin the tank 10 and at the same time this atmosphere may include someof the treating agent which is or has vaporized. The vacuum pumpdischarges the atmosphere through a condenser 86 which will dischargegases to atmosphere through a conduit 88 with the treating agent vaporsbeing condensed to liquid and passing through the conduit 90 to thereservoir or source of supply 58. A vacuum gauge 92 provided on tank 10gives a visual indication of the amount of vacuum within the tank.

Referring now to FIG. 3, a tank is disclosed for receiving arocket-wound package RP. In this embodiment of the invention, the tank10 is modified to provide a stub shaft 100 for reception of the bore atthe nose of the rocket package RP whereas an enlarged collar 102 isprovided for reception of the tail cone 104 of the package RP. The tailcone 104 preferably is perforated or made from a screen material, asshown, so that liquid or vapor can flow easily therethrough.

As hereinbefore mentioned, the systems disclosed in FIGS. 1, 2, or 3 maybe utilized in the batch treatment of textile material or the like withvarious treating agents.

The present invention has been found to yield especially good andunexpected resultsin connection with textile dyeing operations. Theinvention makes it possible to improve many known forms of dyeing.Controlling characteristics or parameters responsible for the success ofthis invention in dyeing operations include the following: providing forextremely rapid flow of the treating agent throughthe textile material,at the very outset of the treating process, whereby treating agent isuniformly distributed substantially in its original concentration andcondition over the surfaces of the textile material to be treated;removal by a strong vacuum (for example, 26-28 inches of mercury, i.e.,24 inches of mercury absolute pressure) in kier 10 of as much air,gasses and vapors from the yarn prior to dyeing as is practical; heatingthe dye bath to the highest practical temperature before adding to thedye kier; pressurizing the dye liquor in tank 16, prior to adding to thedye kier, with a positive pressure of from 0l00 p.s.i. and preferably5075 p.s.i.; and utilizing the high pressure differential between kier10 and tank 16 to force the dye into and through the evacuated yarn. Thesystem is also designed to minimize friction losses in dye liquortransfer by utilizing, as much as possible, large diameter conduits, aminimum number of bends and restrictions, and proper sizing of pumpmeans and valve means, utilizing all desirable engineering practices, aswill be appreciated. Operation of the system may be improved bymaintaining the positive pressure in tank 16 and the vacuum in kier 10during the dye transfer step. And FIG. 4 shows an alternativearrangement wherein a pump 57 is arranged in line 52 between valve 56and vacuum tank or kier 10, to assist in maintaining desired pressure onthe liquor flowing from tank 16 to kier 10.

In the description of the exemplary dyeing operations to follow, it willbe understood that the yarn package (or packages) will be first placedinto the tank 10 as indicated in the drawings. Valve means 56 and thevalve means 74 will be closed. The interior of the tank 10 will then beevacuated or degassed by the vacuum pump 82 until a desired vacuum inthe order of 26-28 inches of mercury is reached (i.e., 2-4 inches ofmercury, absolute pressure). Either simultaneously with the evacuationof the tank or kier 10, or before or after evacuation thereof, the tank16 is filled with dye liquor D to the desired level L by opening thevalve means 66, 70 and 80 and starting the pump 62. When the tank 16 hasbeen filled to its desired level L, valve means 66, 70 and 80 are closedand the dye liquor is then heated to a predetermined temperature asdesired. The dye liquor may be fed directly into tank 16 from othersupply means in any suitable manner, and it may be preheated beforebeing introduced into tank 16, as desired.

The tank 16 may be pressurized during heating of the dye liquor or itmay be independently pressurized. The amount or degree of pressureutilized in the tank 16 is dependent on the type of treatment and howlarge a pressure differential is desired between tanks 10 and 16. Asindicated above, the pressure in tank 16 could range from 0-100 p.s.i.with 50-75 p.s.i. being the preferred range.

The tank 16 may be pressurized independently by opening the valve means34, with the valve means 40 being closed, and flowing air into the tankfrom the source of high pressure air 32 until the desired pressure isindicated on the pressure gauge G.

When the tank 16 has the dye liquor D at the desired temperature andunder the desired pressure, the valve means 34 may be left either openor closed and the quick-opening valve means 56 is opened so that thereis extremely rapid flow of the dye liquor into the bore of the packageand outwardly through the package into the evacuated zone of the tank10.

Valve in vacuum line 84 will be closed during transfer as will beevident. If the FIG. 2 embodiment is used, valve 85" will be closed at asuitable time. The speed of distribution of the dye liquor to thesurfaces of the yarn in the package is substantially instantaneous.

The present invention also contemplates extremely rapid transfer ofsubstantially the entire charge of treating agent in tank 16 to tank 10,through the yarn package. For example, it has been found that when thetank 10 with a package therein is capable of receiving about 5,000 ml ofliquid, it can be filled with this liquid in about one second when ithas been first evacuated to 28 inches Hg. and then placed incommunication with the dye liquor under a positive pressure of 20 p.s.i.Changes in temperature but not in pressure did not materially affect thetransfer time for tests that were made at F, F and 200F. For largerscale operations, utilizing hundreds of gallons of treating agent intank 16, the transfer times were still exceedingly rapid, as will appearfrom the examples given below.

As previously indicated, a vacuum may be maintained in the kier 10during the dye transfer step, after valve 56 is opened, by maintainingvalve 85' in vacuum line 84 open for a suitable time; likewise apositive pressure may be maintained in tank 16 after the valve 56 isopened.

If it is desired to recycle the dye liquor to obtain the desireddiffusion of the dye stuffs from the liquid media into the textilematerial, it is merely necessary to close valve means 56 when all of thedye liquor D is in the lower tank 10, open the valves 74, 70 and 80, anduse pump 62 to pump the dye liquor back into the upper tank 16. Then thesteps of the process are repeated as described above. If it is desiredto recirculate the dye liquor to obtain the desired diffusion of dyestuffs into the textile material, it is merely necessary to allow valvemeans 56 to remain open, open valves 70, 74 and 80 and use pump 62 topump the dye liquor from kier 10 through valves 70, 74 and 80 into uppertank 16 thereby allowing the dye liquor to flow continuously throughconduit 52, package TP, kier l0, tank 16 and back into kier 10, etc. Thedirection of flow for recircu- Iation may be reversed, by reversing theflow through pump 62, to effect outside-in recirculation flow throughthe yarn package.

Valve 85 in vacuum line 84 will be closed during recycling orrecirculation, as will be evident.

In another example of color fixation procedure, the dye liquor isdrained from the lower tank 10 by opening the valves 66 and 74 and whenso drained these valves are closed and the valve means 56 is alsoclosed. The tank 10 is then evacuated by operation of the vacuum pump.The upper tank 16 at this time will be empty and with the valve 80closed and the valve 40 open, steam is supplied to the tank 16 until itreaches a predetermined pressure and temperature. The steam is thenpassed through the yarn package in the same manner as the dye liquor,i.e., by opening the quick-opening valve means 56. Vacuum pump 82 may beallowed to operate (with valve 85 open) during steaming opera tion tofacilitate the transfer of the steam atmosphere through package TP, aswill be appreciated.

The process and apparatus described herein may be used for any batchtype of gaseous or liquid treatment where it is necessary or desired tohave distribution of this treating agent in substantially its originalcondition to all surfaces of the textile material to be treated, and atthe very outset of the treating process for that material. Thus, forexample, it is believed that the invention may be applied to otherprocesses than dyeing, such as mercerizing, scouring, finishing, and thelike. Representative operations, which are given only for the purpose ofillustration, are described in the following three examples wherein thepercentages are on weight of yarn. In each of these three examples, thetime to fill the evacuated chamber with dye liquor was only about onesecond.

EXAMPLE I An 18 ounce tube type of yarn package having 5.5/1rayon/cotton thereon was dyed according to the present invention in avacuum tank having a volume of 5,000 ml. A dye liquor comprising 5percent (OWY) Fastolite Blue BFL and 20 percent (OWY) salt was placed inthe upper tank, referred to as the expansion tank, and was heated toabout 200F. The lid on this tank was then closed and live steam wasadded until a pressure of 40 pounds per square inch was reached.

After the expansion tank 16 was made ready as described, the vacuum tankhaving the package to be dyed therein was evacuated until a reading of28" of mercury was attained. Once this was accomplished and with thelive steam cut off in the expansion tank, the expansion tank was placedin communication with the vacuum tank and the dye liquor within onesecond had transferred from the expansion tank and flooded the vacuumtank. The package was allowed to stand in the dye liquor for 5 minutesand then the dye liquor was discharged from the vacuum tank and thepackage was removed. Careful examination of the package showed that itwas thoroughly impregnated with the dye liquor.

EXAMPLE 2 An 18 ounce yarn package of 5.5/ l rayon/cotton was dyed in avacuum tank having a volume of 5,000 ml. The same steps for dyeing, andthe same dye liquor were used as in Example I; however, additional stepswere tried as follows.

After the package had been let stand for five minutes in the dye liquor,the dye liquor was removed from the vacuum chanber and a vacuum of 28"of mercury was pulled on the chamber for three minutes. The expansiontank utilizing the previously used dye liquor was refilled and reheatedto about 200F. Live steam pressure of 28 pounds per square inch wasapplied to the expansion tank whereas the vacuum tank was then placedunder a vacuum of 26" of mercury. The vacuum tank was placed incommunication with the expansion tank and the dye liquor again floodedthe vacuum tank with the yarn package being allowed to stand in this dyeliquor for five minutes. The dye liquor was then removed from the vacuumtank and a vacuum was pulled for 2 minutes to remove any excess dyeliquor from the yarn of the package.

The package was then removed and examined and it was apparent that theyarn dyed very level and the package looked quite safisfactory.

EXAMPLE 3 A yarn package of percent cotton yarn was dyed in a similarmanner to Example 1. However, in this instance the yarn package was apackage of the type shown in FIG. 2.

Utilizing the same type of dye liquor, same temperatures and pressuresas in Example 1, the yarn package was dyed for five minutes. Uponevaluation of the finished package, it was found that color was veryuniformly distributed throughout the package.

COMBINING OPERATIONS IN THE SAME DYE BATH The concepts of the presentinvention, referred to above, have been found to make it possible tocombine operations, such as scouring and dyeing, in the same dye bathwith improved results, as will be indicated in the following sectionsand examples.

DIRECT DYEING OF CELLULOSIC FIBERS AND YARNS Conventionally, in directdyeing of cellulosic fibers and yarns, a pre-scour is used to removeoil, waxes, and other materials that interfere with even penetration ofthe dye. It was also necessary, by conventional practice, to add thecolor and the salt to the dye bath separately and in small incrementsover a period of about 40 minutes, while the temperature of the dye bathwas slowly raised.

The present invention was applied to the specific area of direct dyeingof cellulosic fibers. An improvement in wetting and levelness of dyeinghas been obtained when air, vapors and other gases were removed from theyarn prior to dyeing simultaneously with the rapid addition of the dyeliquor at high temperature under a positive head of pressure. Some ofthe objectives were:

1. To attempt to reduce the dye cycle time for direct dyeing ofcellulosic fibers and yarns.

2. To attempt the combination of the pre-scour with the dyeing operationin one bath.

3. To bring the dye to temperature with the salt present and theninitiating dye flow through the package to achieve uniform distributionof the dye solution throughout the entire package substantiallyimmediately.

Thus, the mixing of dye, salt, and pre-scour chemicals all in one bathand applying this at high temperature, e.g., about 200F, rapidly to thedry yarn violates principles laid down for obtaining good level dyeingof cellulosic yarns and fiber. Yet, this process of simultaneousscouring and dyeing has been applied to a wide diversity of dyes andcellulosic fibers and yarn types and packages with remarkable success,as illustrated by the following examples.

MPLENQ 1 D REC DXEIN IN .5 POUND PACKAGE DYE MACHINE 50 pound lot on dyesprings Yarn-Rayon Count /1 Color-Blue Dyestuff-Direct In this example,the expansion tank was filled to the desired level and scour chemicals,dye, salt, and dye additives were added. Thereafter, the mixture washeated to 200F. The pressure onthe expansion tank 16 was 50 pounds persquare inch. The kier 10 was evacuated to approximately 26 to 28 inchesof mercury. The drain (or valve 56) was opened to the expansion tank andthe dye liquor was transferred through the packages from the inside-outwith the transfer time for the entire volume of dye liquor being 23seconds.

It was run for 3 minutes inside-out and 7 minutes outside-in. The yarnwas exposed to the dye for 30 minutes at 200F (under 10 to psi.) and thedye bath was thereafter drained. The yarn was thereafter rinsed in anormal manner.

Results Shade satisfactory; Weight heavy; Ap-

pearance satisfactory. Machine Time 1 hour and 30 minutes. EXAMPLE NO.2A DIRECT DYEING IN 50 POUND PACKAGE MACHINE A 51 pound lot on springsYarn-Rayon Count 10/1 Color-Gold Dyestuff-Direct. The procedure used inthis dyeing sv h t dsss ib d nset E am s N9. 1A-

Results Shade satisfactory; Weight satisfactory. Machine Time 1 hour and30 minutes. Example No. 3A Direct Dyeing in 50 Pound Pack age Machine A42 pound lot on dye springs Yarn-Rayon/Cotton Count 7/2 Color-OrangeDyestuff-Direct. This dyeing was also done by the procedure for ExampleNo. lA.

Results Shade satisfactory; Weight satisfactory; Appearancesatisfactory. Machine Time 1 hour.

EXAMPLE NO. 4A

Four Lots were run in a 7 hour period. The procedure described inExample 1A for the 50 pound dye package machine was essentially followedin the production runs except the time for transfer for the entirevolume of dye liquor (from tank 16 to kier l0) was n gw 1 sec.

Second Run 1,972 pounds Yarn-Rayon/Cotton Slub Yarn Color-Direct GreenDyestuff-Direct Results Same as first run.

Machine Time 1 hour and 20 minutes. Third Run 1,903 pounds Yam-KP.Cotton Yarn Count 5.5/1

Color-Direct Green Dyestuff Direct Results Same as two previous runs.

Machine Time 1 hour and 20 minutes. Fourth Run 1,976 poundsYam-Rayon/Cotton Slub Yarn Color-Direct Green Dyestuff-Direct ResultsSame as three previous runs.

Machine Time 1 hour and 20 minutes.

The following tables, in parallel, comparing requirements forconventional direct dyeing with direct dyeing of the present processcombining the dyeing and scouring operations, show advantages of thenovel process disclosed herein.

Conventional Direct Dyeing Direct Dyeing of the Present Process 1.Pre-scour 30 minutes to 45 minutes. No pre-scour 2. Rinse cycle 15minutes 2. Add scour chemicals, dye, salt,

and any other desired chemicals to bath at one time.

4. Total machine time 3 hours 4.

The wide range of cellulosic yarns and direct dyestuffs tried hasdemonstrated that the scope of this invention essentially covers manytypes of cellulosic yarns and fibers and a wide range of directdyestuffs. Specific variables are as follows:

The pressure range for transfer of the dye to the dye packages can be0-100 p.s.i., but the preferred range is 50 to 75 pounds per squareinch. The actual dyeing is carried out at a pressure of 0 to 30 psi.with a preferred range of 10 to 20 psi. The dye package is evacuatedwith the lowest practical pressure obtainable in the dyeing equipment.In practice, this has proved to be about 26 to 28 inches of mercury.Preferred temperature range is 160F to 200F, although the temperaturecan go higher, if desired.

Naphthol Dyeing of Cellulosic Fibers and Yarns has to be very carefullycontrolled in order to get good uniformity in the shade of the dyedyarn. It also requires that the coupling agent penetrate the yarnrapidly and evenly so that the degree of reaction is uniform throughoutthe yarn package. Shading to produce the desired color is difficult withthe developed colors because in many cases the developed color issufficiently different from the initial color (after the naphtholatestep) on the cloth or yarn that a great deal of experience is necessaryto be able to obtain the proper shade.

It has been found that the application of vacuum during the couplingstep increases the speed of penetration of the solutions into the yarnand brings about uniform and complete reaction of the two dyecomponents. This has resulted in reducing the amount of reworking of dyelots to obtain the proper shade. The novel system and techniques,referred to herein, also appear to reduce the tendency of naphthols tocrock.

The examples given below illustrate dyeing of cellulosic yarns withvarious naphthol dyes.

Example No. 1B Dyeing of Cellulosic Yarns by Naphthol Dyes in VacuumPackage Dyeing Equipment A 45 pound lot of yarn on dye springs YarnCotton Count 5.5/1

Color Red Dyestuff-Naphthol Dye Dyebath:

1.0 percent Sycopen 0.5 percent Chelate 3.0 lb. caustic soda (50 percentvol.) 8.6 percent Naphthol ASSW (33 percent vol.) 0.5 percent CasolineOil 2.0 percent Methanol 0.36 percent Naphthol ASLB (20 percentsolution) 2 salt rinses (2.5 gal. brine) Coupling Bath:

3.2 percent Fast Red PDC Base 0.5 percent Triton X405 4.0 percentMuriatic Acid 1.6 percent Sodium Nitrate 3.2 percent Sodium Acetate 2.0percent Acetic Acid Scour No. l: 1.0 percent Triton X405 Scour No. 2:1.0 percent Bi-scour D 1.5 percent Soda Ash Sofetener: 1.5 percentSouravel DYEING OF CELLULOSlC FIBERS OR YARNS WlTH NAPHTHOL DYES 1. Fillexpansion tank and heat to 140F.

2. Add caustic soda while circulating.

3. Add salt while circulating.

4. Cut off pump and add boilout.

5. Start pump and add naphtholate.

6. Transfer dye to kier and run at 160F for 20 minutes with transfertime for the entire volume of dye liquor being 23 seconds.

7. Cool to 100F and run minutes. Drain.

8. Run first salt rinse from big expansion tank with 30 pounds causticsoda (50 percent).

9. Run second salt rinse by regular production procedure.

l0. Vacuum extract twice.

1 1. Mix base (add ice only in summer) in big expansion tank andtransfer to kier and run 30 minutes at 60-70F. Drain.

12. Add first scour and run at 130F for 10 minutes.

Drain.

13. Hot wash continuously inside/out until clear.

14. Add second scour and run at 200F for 10 minutes. Drain.

15. Hot wash continuously inside/out until clear. Results The shade wassatisfactory. A good level dyeing was obtained throughout the package. Areduction in crocking was noted.

Machine Time 4% hours. Example No. 2B Dyeing of Novelty Rayon Yarn byNaphthol Dye in Vacuum Package Dyeing Equipment 20 pound lot novelty yamon dye tubes Yarn-Novelty Rayon ColorC/Red Dyetsuff-Naphthol DyeDyebath:

0.5 percent Chelate No. 1 7.0 percent Caustic Soda (50 percent vol.) 8.0percent Naphthol ASSW (33 percent vol.) 0.33 percent Naphthol ASLGpowder 0.9 percent Naphthol ASLB powder 0.5 percent Caustic Soda 4.5percent Methanol 0.5 percent Triton X405 0.2 percent gal. salt brineCoupling:

2.4 percent Fast Red KB Base 0.5 percent Triton X405 2.4 percentMuriatic acid 1.20 percent Sodium Acetate 0.96 percent Sodium nitrateScour No. l: 1.0 percent Triton X405 Scour No. 2: 1.0 percent Soda Ash l1.0 percent Triton X405 The same procedure was used in running this dye-1 ing as was used in Example No. 18 above. Results Shade wassatifactory. A good level dyeing was obtained throughout the package.

Specific variables of the above process of naphthol dyeing include thefollowing: pressure range for transfer of dye to dye package can be0-100 p.s.i., but the preferred range is 50 to p.s.i.; the actual dyeingis carried out at pressures of 0 to 30 p.s.i. with a preferred range of10 to 20 p.s.i.; the dye package is evacuated to the lowest practicalpressure obtainable in the dye equipment and, in practice, this provedto be 26 to 28 inches of mercury; and preferred temperature range is Fto 180F.

Some advantages realized in the application of the invention to naphtholdyeing are as follows: no prescour is required; scouring chemicals anddye can be added in one bath and both operations can be performedsimultaneously; substantial savings in water usage; time for thenaphtholate procedure is reduced approximately one-fourth; theuniformity of naphthol dyeings is improved by using vacuum to impregnatethe package with coupling salt; and the total time for the naphtholdyeing cycle has been decreased from 7 hours to 4% hours.

Vat Dyeing of Cellulosic Fibers and Yarns The principal problems ofdyeing cellulosic fibers and yarns by the vat procedure stem from thecomplex multistep process required and from the fact that the method hadto be varied from one vat color to another.

Such changes in the methods or procedures may lead to confusion anderror when changing from one vat dyeing to another, as will beappreciated. The use of the method of this invention for adding the dyesubstantially reduces the time for impregnation of the yarn. Thecompleteness of impregnation has also improved the levelness of dyeing.The experience to date indicates that one dyeing procedure can beapplied to many vat colors. This would simplify the training of dyersand would also minimize the danger of poor dyeing results due to choiceof the wrong method. The total process time for vat dyeing has beenreduced, by this novel method, by about 25 percent.

The novel methods, referred to herein, of vat dyeing of cellulosicfibers and yarns have been found to permit realization of the followingobjectives: simplification of the dyeing process; improvement of theevenness of impregnation of the dye package with the dispersed vat dyeparticles; reduction of the variation of procedure heretofore necessaryfor virtually each vatdye; and development of a better procedure forunion dyeing polyester/cotton blends.

The following examples illustrate application of the invention to thedyeing of cellulosic fibers and yarns, and blends, with vat dyes.

Example No. 1C Dyeing of Polyester/Rayon Yarn Using Vat Dyes for theRayon An 84 pound batch of yarn was dyed:

Fibers 65/35 Fortrel/Rayon Color-Gold Yarn Count 21/2 Results Laboratoyevaluation of this dyeing was satisfactory and the dyeing was on shade.

Machine Time Conventional dyeing time 275 minutes running time. VacuumDyeing time 215 minutes.

Vat Dyeing of Cotton 1. Evacuate kier 10 minutes.

2. Add 'dye and auxiliaries to expansion tank.

3. Pressurize expansion tank to 40 p.s.i.

4. Transfer dye to kier on inside/out with transfer of total volume ofdye liquor from tank 16 to tank 10 taking 18 seconds.

5. Switch to outside/in-run 10 minutes.

6. Add caustic soda run minutes.

7. Add sodium hydrosulfite run 20 minutes.

8. Rinse for 20 minutes.

9. Add sodium perborate, heat to 160 F, then add soap and heat to 200F.

10. Run for minutes.

1]. Rinse 20 minutes.

12. Add finish and run minutes.

13. Drain.

Example No. 2C Fortrel/Cotton Dyeing An 84 pound load of the followingyarn was vacuum dyed:

Fibers 50/50 Fortrel/Cotton Color-Dahlia Yarn Count 31/2- Results Lusterof this dyeing was satisfactory and uniform result was noted from theknitted sock. The shade matched the control shade. Four dyeings usingtwo-ply yarn produced excellent uniformity.

Machine Time Conventional dyeing time Approximately 300 minutes. Vacuumdyeing time 210 minutes.

The procedure used for this dyeing was the same as given in Example No.1C. Example No. 3C Fortrel/Cotton Dyeing A pound load of the followingyarn was vacuum dyed: Fibers 50/50 Fortrel/Cotton Color-Pink Yarn Count21/1 Results Luster was satisfactory and levelness and uniformity weregood. Machine Time 300 minutes, Vacuum dyeing 215 minutes.

The same procedure was used for this dyeing as was used in Example No.1C. Example No. 4C Dyeing Polyester/Cotton Yarn with Problem Vat ColorsThree vat colors which had been problem shades when dyed on 50/50Fortrel/Cotton by conventional pressure dyeing were successfully dyedaccording to the present invention. The procedure used was the same aswas given in Example No. 1C above, and the yarn count on this blend was31/1. The colors dyed in successive runs were Grey; Gold; and Blue. Ineach case, use of the techniques of the present invention gave excellentlevel and uniform dyeing, as was shown by examination of the knittedsocks and the shade was a good match to the control. The machine time ineach of these cases was 215 minutes as opposed to a normal machine timeof 275 minutes. Example No. 5C Dyeing Procedure for Applying VatDyestuff to Percent Cotton and Rayon/Cotton Yam 1. Premix dye withBiChem Dyebath PR-50 and Chelate No. l. 2. Fill expansion tank todesired level and heat to F F. Add dye to expansion tank. 3. Pressurizeexpansion tank to 55 p.s.i. and pull vacuum on kiers. 1. Transferdyebath to kiers, with transfer time for the entire volume of the dyeliquor from tank 16 to tank 10 being 18 seconds. Run 30 seconds inside/-out. 5., Run outside/in for 15 minutes. Release air pressure. 6. AddBasogal P andcaustic soda, run 10 minutes. 7. Add sodium hydrosulfite inthree parts at 5 minute intervals. 8. Run 30 minutes. 9. Start coldrunning wash outside/in and cool to 100F. 10. Switch to inside/out andwash until clear (2030 minutes). 11. Add sodium perborate or hydrogenperoxide and raise temperature to 200F. 12. Add scouring chemicals andrun 15 minutes. 13. Start hot running wash inside/out and run untilclear. Cool to 100F and drain. This dyeing was made on 1,130 pounds ofcotton. Fibers KP Cotton ColorVat Orange Yarn Count 5.5/1 Results Auniform and level dyeing was obtained throughout all the packages. Thecolor was on shade with the control. Machine Time 215 minutes. ExampleNo. 6C Vat Dyeing of Rayon/Cotton Slub The dyeing procedure was the sameas given in Example No. C, above. The kier was loaded with 1,198 poundsof Rayon/Cotton.

Fibers Rayon/Cotton Slub Color Vat Orange Results A level dyeing wasobtained with good uniformity throughout the yarn packages. Dyeing wason shade with the control.

Machine Time Approximately 215 minutes.

Specific variables of the vat dyeing processes are essentially the sameas those previously given regarding pressures and temperatures in thetanks l0, 16.

Some of the advantages from application of the novel methods disclosedherein to vat dyeing of cellulosic fibers and yarns are as follows:

1. Makes it possible to dye polyester/cotton yarns and fibers with manydifferent dyes using simplified procedures. In contrast, different vatcolors heretofore required variations in the dyeing procedure.

2. ln dyeing cotton and cotton/rayon blends, the boilout chemicals canbe added directly to the dye bath.

3. Additions of certain chemicals to the dye bath can be made at thebeginning of the dye cycle.

4. The rapid wet-out of the yarn in the present invention makes itpossible to add these chemicals in one step.

5. Satisfactory uniformity of distribution of the dye throughout thepackage is achieved in a simplified procedure.

6. The variation of shade from package to package for those on the topof the dye stand to those at the bottom is virtually eliminated due tothe excellent wet-out obtained by the impregnation of the dye packages.

Dyeing of Polyester and Polyester Blends There has been an increase inthe use of polyester fibers alone and as blends with natural fiberswhich has made it desirable to reduce the length of time necessary todye polyester. This need resulted in application of the invention topolyester dyeing and advantages have been realized by the use of thissystem rather than the conventional or normal pressure dyeing method, aswill become evident. With respect to 100 percent filament polyesteryarn, other objectives, besides reducing the cycle time, were toeliminate any need for preautoclaving polyester yarn to heat-set itbefore dyeing, and to improve the shade uniformity of polyester dyemg.

It will be understood that there are two dyeing procedures for dyeingpolyester/cotton blends, one to dye the polyester portion and one to dyethe cotton. The following examples are concerned only with the dyeing ofthe polyester portion:

Example-No. 1D Dyeing of Polyester in a Modified 100 No. Package DyeingMachine Yarn-84 lbs. of polyester/cotton Fibers 50/50 Fortrel/CottonColor-Olive Yarn Count 35/1 Procedure used to run polyester part of theyarn as follows:

1. Fill expansion tank at 180F, add pre-scour chemicals, carrier andother chemicals and dye. Pressurize the expansion tank to 50 p.s.i.

2. Evacuate kier to approximately 26-28 inches mercury.

3. Set controller temperature to 255F and rate rise to maximum4-5F/minute.

4. Open expansion tank drain and the entire amount of dye liquor wastransferred to the vacuum tank in 23 seconds. Run for 3 minutesinside/out, 3 minutes outside/in.

5. When temperature reaches 255F, run for 30 minutes and drain at 200F.

6. Wash with hot water until clear.

Results Luster was satisfactory, uniformity of dyeing was excellent andthe woven fabric looked very good. Machine Time Standard or conventional(nonvacuum) Dyeing Time 110 minutes. Vacuum Dyeing minutes running time.

Example No. 2D Dyeing of Polyester in Modified No. Package DyeingMachine Yam-Po1yester/Rayon Color-Black Yarn Count 14/1 Dye procedure ofExample No. ID was used to dye this yarn as well.

Results Luster was satisfactory and the uniformity of dyeing wasexcellent. The lot of yarn was used as filling yarn and woven intofabric. Observations on the inspection table showed that all the vacuumdyed yarn was of first quality and gave a brighter black than theportion of the cuts with regular black yarn.

Machine Time 70 minutes running time vs. 1 10 minutes running time ofthe standard or conventional (nonvacuum) dyeing procedure.

Example No. 3D Package Dyeing of Polyester Tow A l-pound lot ofpolyester tow was dyed according to the invention, using the procedureof Example No. 1D.

Yam-T-64 Crimped Dacron Polyester tow Color-Three dyeings were carriedout with the following colors: Rust; Blue and Green.

Dyestuffs-Disperse Results Repeatability of dyeing was good, levelnessof dyeing was good, and pictures, micro-photographs of the textilematerial showed good penetration with no evidence of ring dyeing.

Machine Time Regular or conventional (nonvacuum) Process 3% hours vs.Vacuum-Pressure Method 1% hours to 1% hours.

Example No. 4D Package Dyeing of Textured Polyester The procedure ofExample No. ID was used in this example also. Two 1 pound packages oftextured polyester yarn were dyed one was autoclaved and the other wasnot.

Yarn-Textured Polyester /34, T-56 Color Yellow Dyestuff-Disperse ResultsYarn was knitted into sleeves, all of which showed very level dyeing. Itwas impossible to tell the difference between the autoclaved andnonautoclaved yarn on the basis of this dyeing. Machine Time 1% hours to1% hours. Example No. 5D Package Dyeing of 100 Percent TexturedPolyester Fabric The dyeing procedure of Example No. ID was used in thisexperiment. A sleeve of polyester double knit weighing 390 gms. was puton'the dye spindle.

Yam-100 percent Textured Polyester Color Green. Results Good leveldyeing was obtained. Machine Time 1 hour 20 minutes. Example No. 6DDyeing of Textured Polyester Yam Packages This example was carried outaccording to the procedure of Example No. lD. Repeat dyeings were madein one pound lots on textured polyester yarn two Rose Quartz, threeRegal Purple, and two Expresso.

Yarn-Textured Dacron Polyester T-- 56 Denier 150/34 Color--Rose Quartz,Regal Purple, and Expresso DyestuffDisperse 7 Results There was gooduniformity from one dyeing to another of each shade.

Machine Time i k hours.

The foregoing examples indicate that the invention can be applied totextured and untextured, spun and filament polyester and polyester tow.Specific variables include: pressure range to transfer the dye to thedye packages is essentially to 100 p.s.i., but the preferred range is 50to 75 p.s.i.; the actual dyeing is carried out at a pressure of 0 to 30p.s.i. with the preferred range of 10 to p.s.i.; the dye package isevacuated to the lowest practical pressure obtainable in the dyeequipment and, in practice, this has proved to be 26 to 28 .inches ofmercury. Preferred temperature range is 180F to 255F.

The following parallel tables indicate the advantages of dyeingpolyester by the novel methods disclosed herein, as compared to standardor conventional methods:

Standard Pressure Polyester Dyeing Vacuum-Pressure Polyester Dyeing l.Yarn is autoclavcd prior to dyeing to heat-set it.

. It is not necessary to pre-autoclave the polyester yarn.

2. A pre-scour of about 45 minutes is run. 2. The pre-scour of the yarnhas been eliminated.

3. The dyeing cycle requires about 3 to3'k hours.

. The dyeing cycle has been reduced from about 3 to 3% hours to about 1hour 10 minutes to 1 hour and 30 minutes. Securing and dyeing arecarried out simultaneously in the same bath.

4. Considerable difficulty is encountered in obtaining shade uniformity.4.ln the normal procedure the dye bath starts out at a low temperatureof about 100F and is raised slowly to an optimum of 230-255F in order toget level dyeing. However, it is possible to apply the dye bath at l80F-l90F to the dry yarn and raise the temperature at a rapid rate to255F.

5. Much better uniformity of shade has been obtained.

DYEING WOOL Conventional dyeing of wool yarns and tops made from wool orwool blends has been beset with four primary problems: (1) Hightemperature used in dyeing these fibers has caused loss of strength andelongation; (2) Pressure buildup due to the slow wetting and penetrationinto the top and yarn package has caused blowing of tops with subsequentnecessary reworking and tremendous dollar loss due to felted wool; (3)

Poor uniformity of shades within dye package due to uneven striking ofthe dye into the yarn package; and (4) Felting due to prolonged exposureto circulation of dye liquor. The application of the novel methodsdisclosed herein to the dyeing of wool and wool blends has been found toeliminate or minimize these problems, and to realize the followingobjectives: reduction of the time necessary to dye wool andwool/polyester blended yarn; reduction of the time at temperaturenecessary to obtain good level dyeing of wool and wool blends by takingadvantage of the superior wetting and penetration due to the evacuationof air; reduction of wool felting during dyeing; and reduction of thetime necessary to dye wool thereby reducing the damage done to thephysical properties of wool yarn.

The following examples illustrate application of the novel methodsdisclosed herein to dyeing wool top, percent wool and wool/polyesterblended yarn. Example No. 1E Grey 0.5 percent Nonionic detergent 0.75percent Acetic Acid 0.1 percent Chelate No. l

1.0 percent BiChem Dyebath DA 0.4 percent Isolan Black GLVacuum-Pressure Procedure for Wool Top l.Pull vacuum for 10 minutes onkier.

2. Set temperature control at 190F for Grey.

3. Fill expansion tank with dyebath including acid and dyestuffauxiliaries at 190F.

4. Close expansion tank lid and heat to 5 p.s.i. steam.

Add air to total 50 p.s.i.

5. Transfer dyebath to the dye kier on an inside/out setting withtransfer time being 4 seconds for transferring 7.5 liters from theexpansion tank 16 to the vacuum tank 10. Switch to outside/in.

6. Run for 2 minutes inside/out and 3 minutes outside/in.

7; Run for 20 minutes.

8. Cool to F and drain.

9. Cold wash inside/out.

Results Uniformity of dyeing was good. There was less loss of strengthand elongation of wool fibers. Machine Time 45 minutes rather than 200minutes normal production time.

Example No. 2E Gold 0.5 percent Nonionic detergent 1.5 percent Aceticacid 0.5 percent Chelate No. l

1.0 percent BiChem Dyebath DA 2.65 percent lsolan Yellow GSA 0.38percent Levolan Brown lBRL The same vacuum dyeing procedure was used aswas given in Example No. 1B, except the dyeing temperature was 200F forthe Gold Color.

Example No. 3E Vacuum Dyeing vs. Regular or Conventional Production Yarnl/50 Wool Color Gold Two cones of H50 wool yarn were vacuum dyedaccording to the invention. This data was compared with regularproduction data from the same color, gold. The procedure used in dyeingthese lots was the same as given in Example No. 1B above, except thedyeings were made at two different temperatures, 200F in one lot and210F in the second lot. Dyeing time was 15 minutes on each pulse time toprepare for dyeing and to wash at the end of the dye cycle. Thefollowing table gives test data on these two vacuum dyeing runs comparedwith regular plant dyeings over a three month period of the same colorgold.

3 Months Regular Dyeing of Vacuum Dyeing Color Gold 200F 210F Dyed yarnstrength grams 123.0 108.8 129.8 121.4 126.4 115.1 83.0 elongation 11.08.6 l 1.1 9.9 l 1.0 9.3 7.4 Natural yarn lot 5012 yarn strength. grams97.3 97.3 (Other lots) elongation 9.3 9.3 Extractablcs oil extractable3.95 3.91 alcohol extract- 1.20 1.20 able water Extractable 0.04 0.04acid scour 1.85 1.51 Total extractables 7.04 6.65 Chemical tests pH 4.44.5 Full and scour 4.7 4.0 4.5 Crabbing 4.5 4.3 4.4 Sublimation 5.0 5.0Blank neutral 2.8 2.3 2.8 Blank polyester 2.8 2.3 2.6 Acid perspiration4.5 4.5 4.8 Alkaline perspira- 4.0 4.0 4.6 tion Dry cleaning 50 5.0 4.6Lightfastncss (Break at) 60 hrs. 60 hrs. 60 hrs. (very slight) (Slight)(very slight) It might be noted that the improvement in strength andelongation after dyeing did not adversely affect the other properties ofthe wool.

Machine Time 45 minutes vs. 135 minutes for conventional or standardproduction time.

Example No. 4E Dyeing of Wool Top with Premetallized Dye Grey 1. Dye,chemicals, and other ingredients were added to the expansion tank andheated to 150F.

2. Expansion tank lid was closed and pressurized to 30 p.s.i.

3. Kier evacuated at 26-28 inches mercury.

4. Open expansion tank drain and transfer the entire volume of dyeliquor from the tank 16 to tank in 4 seconds. Start pump on inside/out.After 1 minute switch to outside/in.

5. Raise temperature to 200F.

6. Run 30 minutes drain.

7. Rinse Results Uniformity of dyeing was good.

Machine Time 45 minutes rather than 135 minutes normal production time.

Controlling characteristics which have been found to make it possible toimprove dyeing of wool top, 100 percent wool and polyester/wool blendedyarn are essentially the same as those previously noted and include:

1. Removal of air to the lowest practical vacuum (26-28 inches ofmercury) in the kier;

2. Heating the dye bath to the highest practical temperature (230F)before adding to the dye kier; and

3. Forcing the hot dye into the evacuated yarn under a positive pressurepreferably 50 75 p.s.i.

Some of the advantages realized from application of this invention todyeing wool top, 100 percent wool and wool/polyester yarns are asfollows: (1) No pre-scour is necessary as the lubricating oils can beleft on the wool because they do not interfere with dye penetration intoan evacuated yarn. (2) Dyestuff auxiliaries and acid can be placed inone bath. (3) Dye is entered into the yarn at dyeing temperature. (4)Excellent levelness throughout the dye package is obtained in dyeingwool and wool blend yarns. (5) Reduction in the time the wool yarn isheld at a high temperature minimizes strength loss and reduces yarnshrinkage, improves elongation and reduces felting as compared withnormal dyeing. (6) Machine time is reduced from minutes to 45 minutes.

TRANSFER TIMES In some of the above examples, times were given for therapid transfer of the dye liquor or charge from the expansion tank 16 tothe kier or vacuum tank 10. The following is an exemplary table of suchinformation, derived from application of the present invention indifferent installations:

Installation No. Volume Transferred Time 1. 1,100 gal. 18 sec. 2. 800gal. 16 sec. 3. 800 gal. 16 see. 4. 960 gal. 26 sec. 5. 960 gal. 16 sec.6. 980 gal. 45 see. 7. 7.5 liters 4 see.

It will thus be seen that the objectives, noted above, have beenaccomplished.

As will be evident from the foregoing, the time for transfer of theentire charge of treating agent from the expansion tank 16 to the vacuumtank 10 is a different parameter from the time it takes for uniformdistribution of the treating agent over the surfaces of the textilematerial being treated and at the outset of the process. The latter timeperiod is terminated substantially immediately after the textilematerial is first contacted by the treating agent. The former timeperiod is terminated sometime after that.

The terms surfaces of the textile material" or surfaces of the yarn orthe like, as used herein, should be understood to include the surfacesof the fibers comprising the textile material being treated inasmuch asresults indicate and it is believed that there is a uniform distributionof the treating agent over all or substantially all of the surfaces ofsuch fibers substantially immediately after the textile material beingtreated is first contacted by the treating agent.

I claim:

1. In a process for the batch treatment of textile material with aliquid treating agent including a dye liquor, the improvementcomprising: placing the textile material to be treated in an enclosedfirst zone and applying a substantial vacuum in the range of 0 10 inchesof mercury, absolute pressure, to the first zone to produce a greatlyreduced sub-atmospheric pressure therein; providing the liquid treatingagent in a second zone and heating it therein, placing the treatingagent in said second zone under a positive pressure at least as great asatmospheric pressure; placing the first zone in communication with thesecond zone through a relatively large diameter conduit; and effecting avery rapid initial transfer of said treating agent from said second zonethrough said conduit and into said first zone wherein said treatingagent flows through said textile material in an inside-out direction,said transfer taking place at a flow rate of at least about 750 gallonsof said treating agent per minute so that said treating agent isuniformly distributed over all or substantially all of the surfaces ofsaid textile material substantially immediately after the textilematerial is first contacted by said treating agent and so that saidsurfaces-of said textile material are initially exposed to or wetted bythe treating agent at uniform or substantially uniform concentration ofsaid dye liquor.

2. The process defined in claim 1 including subjecting said agent to apredetermined superatmospheric pressure while in said second zone.

3. The process defined in claim 1 wherein the pressure in the secondzone is 75 p.s.i., and wherein the vacuum in said first zone isapproximately 26 28 inches of mercury, i.e., about 2 4 inches of mercuryabsolute pressure.

4. The process defined in claim 3 wherein the treating agent is heatedto approximately 160F. 220F. while in said second zone and prior totransfer into said first zone.

5. The process defined in claim 4 wherein the treating agent issubjected to a positive pressure of about 50 75 p.s.i. while in saidsecond zone and prior to transfer into said first zone.

6. The process defined in claim 3 wherein the textile material comprisescellulosic fibers.

7. The process defined in claim 3 wherein the textile material comprisespolyester.

8. The process defined in claim 3 wherein the textile material compriseswool.

9. The process defined in claim 1 wherein both the vacuum in the firstzone and the positive pressure in said second zone are maintained duringthe step of transferring the treating agent between the zones.

10. The process defined in claim 1 including isolating the second zonefrom the first zone after the treating agent has flooded the first zoneand then flowing the treating agent from the first zone.

11. The process defined in claim wherein the cycle of operation offlooding the first zone with the treating agent isrepeated.

12. The process defined in claim wherein substantially the entire chargeof treating agent in said second zone is transferred through the textilematerial and into said first zone in a range of about 0 30 seconds afterthe two zones are placed in communication with each other, and furtherwherein the volume of said entire charge of treating agent is at leastabout 750 gallons.

13. The process defined in claim 12 wherein the volume of the entirecharge of treating agent is over about nine hundred gallons, and whereinsaid entire charge is transferred from said second zone into said firstzone in less than about seconds.

14. in a process for batch treating of textile material with a liquidtreating agent including a dye liquor, the improvement comprising:placing the textile material to be treated in an enclosed first zone andapplying a substantial vacuum in the range of 0 10 inches of mercury,absolute pressure, to the first zone to produce a substantial negativepressure therein; providing the liquid treating agent in a second zone;heating the treating agent to a predetermined temperature while in thesecond zone and subjecting the heated treating agent to asuperatmospheric pressure in the second zone; placing the first zone incommunication with the second zone; effecting a very rapid initialtransfer of said treating agent from said second zone into said firstzone wherein said treating agent flows through said textile material inan inside-out direction, said transfer taking place at a flow rate of atleast about 750 gallons of said treating agent per minute so that saidtreating agent is uniformly distributed over all or substantially all ofthe surfaces of said textile material substantially immediately afterthe textile material is first contacted by said treating agent and sothat said surfaces of said textile material are initially exposed to orwetted by the treating agent at uniform or substantially uniformconcentration of said dye liquor; flooding said first zone with thetreating agent; isolating the second zone from the first zone after thetreating agent has flooded the first zone and then flowing the treatingagent from the first zone; reevacuating the first zone after thetreating agent is flowed from the first zone to provide a negativepressure therein; filling the second zone with a second treating fluidunder pressure; and placing the first zone into communication with thesecond zone to cause rapid transfer of said second treating fluid overthe surfaces of the textile material and into the first zone.

15. In a process for batch treating of textile material with a liquidtreating agent including a dye liquor, the

improvement comprising: placing the textile material to be treated in anenclosed first zone and applying a substantial vacuum in the range of 010 inches of mercury, absolute pressure to the first zone to produce asubstantial negative pressure therein; providing the liquid treatingagent in a second zone; heating the treating agent to a predeterminedtemperature while in the second zone and subjecting the heated treatingagent to a superatmospheric pressure in the second zone; placing thefirst zone in communication with the second zone; and effecting a veryrapid initial transfer of said treating agent from said second zone intosaid first zone wherein said treating agent flows through said textilematerial in an inside-out direction, said transfer taking place at aflow rate of at least about 750 gallons of said treating agent perminute so that said treating agent is uniformly distributed over all orsubstantially all of the surfaces of said textile material substantiallyimmediately after the textile material is first contacted by saidtreating agent and so that said surfaces of said textile material areinitially exposed to or wetted by the treating agent at uniform orsubstantially uniform concentration of said dye liquor; flooding saidfirst zone with the treating agent; isolating the second zone from thefirst zone after the treating agent has flooded the first zone and thenflowing the treating agent from the first zone; flowing the treatingagent removed from the first zone back into the second zone; heating andpressurizing the treating agent in the second zone to a predeterminedtemperature and pressure respectively; evacuating the first zone of theatmosphere therein; and then placing the first zone into communicationwith the second zone to cause recycling of the treating agent from thesecond zone through said textile material into the first zone.

16. The process defined in claim 1 wherein substantially the entirecharge of treating agent in said second zone is transferred through thetextile material and into said first zone extremely rapidly.

17. The process defined in claim 16 wherein substantially the entirecharge of treating agent insaid second zone is transferred through thetextile material and into said first zone is a range of about 0 45seconds.

18. The process defined in claim 1 wherein the treating agent isrecirculated between the second and first zones and through the textilematerial.

19. The process defined in claim 1 wherein in said initial transfersubstantially the entire charge of treating agent in said second zone istransferred through the textile material in one direction and into saidfirst zone extremely rapidly, and wherein the flow of the treating agentis thereafter reversed to pass through the textile material in theopposite direction.

20. The process defined in claim 19 wherein in said initial transfersubstantially the entire charge of treating agent in said second zone istransferred through the textile material in said one direction and intosaid first zone in a time period of less than about 45 seconds.

21. The process defined in claim 20 wherein the direction of flow isreversed after about 30 seconds.

22. The process defined in claim 20 wherein the charge of said treatingagent is at least about 800 gallons.

23. The process defined in claim 20 wherein said time period is nogreater than about 30 seconds.

24. The process defined in claim 1 wherein the textile material includesa yarn package in the form of yarn wound on a fluid pervious tube, andfurther wherein the flow of said treating agent through said textilematerial is in a controlled direction wherein the treating agent isconstrained to flow from the interior of said yarn package outwardlythrough the yarn.

UNITED STATES PATENT OFFICE CERTIFICATE OI CORRECTION Patent No. 3,775,55 Ilated N v m r 27, 973

Inventor-(x) Frederick C. Wedler It is certified that error appears inthe above-identified patent and that said Letters Patent are herebycorrected as shown below:

Column 1, line 65, ""the" (second occurrence) should be --The--.

Column 7, line 66, change "chamber" to --chamber--.

Column 8, line 15, change "safisfactory" to --satisfactory--.

Column 11, line &2,- change "Sofetener" to -Softener-.

Column 12, lines 12-13. I These lines should be merged so as to read--Naphtho1 Dye in Vacuum Package Dyeing Equipmen Column 12, line 17,change "Dyetsuff" to --Dyestuff--. Column 12, line 39, change 'sadzifactory" to --satisfactory--.

Column 13, line 33, change "Laboratoy" to Laboratory.

Column 15, line 58 and Column 16, line 18, delete No. and replace with--Pound- Column 18, 1155.66, change "pulse" to plus- Column 19, linesll, 13 and 21, insert underlinings in the first two columns, as theyappear in the original, typed specification.

Column 20, line snjc ha "o 10" to -about 2 4- FORM PO-1050 (10-69)UJCOMM-DC noun-mm h u s. oovllmnnu "mum. mnu luv u u. an

i Page 2 UNITED STATES PATENT OFFiCfE (IERTIFICATE 0F CQRRECTIONInventoflsb Frederick C. Wedler It is certified that error appears inthe above-identified patent and that said Letters Patent are herebycorrected as shown below:

Column 21, lines 12-15, delete and wherein the ar;soI!. 1 1i;e L-pressure."

' 001mm 21 lin 1 selwumniae g, an to Signed and sealed this 21st day ofMay 1974 (SEAL) Attest:

C. MARSHALL DANN EDWARD M.FLETCHER,JR.

Commissioner of Patents Attesting Officer F ORM PC4050 (10-69)

2. The process defined in claim 1 including subjecting said agent to apredetermined superatmospheric pressure while in said second zone. 3.The process defined in claim 1 wherein the pressure in the second zoneis 0 - 75 p.s.i., and wherein the vacuum in said first zone isapproximately 26 - 28 inches of mercury, i.e., about 2 - 4 inches ofmercury absolute pressure.
 4. The process defined in claim 3 wherein thetreating agent is heated to approximately 160*F. - 220*F. while in saidsecond zone and prior to transfer into said first zone.
 5. The processdefined in claim 4 wherein the treating agent is subjected to a positivepressure of about 50 - 75 p.s.i. while in said second zone and prior totransfer into said first zone.
 6. The process defined in claim 3 whereinthe textile material comprises cellulosic fibers.
 7. The process definedin claim 3 wherein the textile material comprises polyester.
 8. Theprocess defined in claim 3 wherein the textile material comprises wool.9. The process defined in claim 1 wherein both the vacuum in the firstzone and the positive pressure in said second zone are maintained duringthe step of transferring the treating agent between the zones.
 10. Theprocess defined in claim 1 including isolating the second zone from thefirst zone after the treating agent has flooded the first zone and thenflowing the treating agent from the first zone.
 11. The process definedin claim 10 wherein the cycle of operation of flooding the first zonewith the treating agent is repeated.
 12. The process defined in claim 1wherein substantially the entire charge of treating agent in said secondzone is transferred through the textile material and into said firstzone in a range of about 0 - 30 seconds after the two zones are placedin communication with each other, and further wherein the volume of saidentire charge of treating agent is at least about 750 gallons.
 13. Theprocess defined in claim 12 wherein the volume of the entire charge oftreating agent is over about nine hundred gallons, and wherein saidentire charge is transferred from said second zone into said first zonein less than about 20 seconds.
 14. In a process for batch treating oftextile material with a liquid treating agent including a dye liquor,the improvement comprising: placing the textile material to be treatedin an enclosed first zone and applying a substantial vacuum in the rangeof 0 - 10 inches of mercury, absolute pressure, to the first zone toproduce a substantial negative pressure therein; providing the liquidtreating agent in a second zone; heating the treating agent to apredetermined temperature while in the second zone and subjecting theheated treating agent to a superatmospheric pressure in the second zone;placing the first zone in communication with the second zone; effectinga very rapid initial transfer of said treating agent from said secondzone into said first zone wherein said treating agent flows through saidtextile material in an inside-oUt direction, said transfer taking placeat a flow rate of at least about 750 gallons of said treating agent perminute so that said treating agent is uniformly distributed over all orsubstantially all of the surfaces of said textile material substantiallyimmediately after the textile material is first contacted by saidtreating agent and so that said surfaces of said textile material areinitially exposed to or wetted by the treating agent at uniform orsubstantially uniform concentration of said dye liquor; flooding saidfirst zone with the treating agent; isolating the second zone from thefirst zone after the treating agent has flooded the first zone and thenflowing the treating agent from the first zone; reevacuating the firstzone after the treating agent is flowed from the first zone to provide anegative pressure therein; filling the second zone with a secondtreating fluid under pressure; and placing the first zone intocommunication with the second zone to cause rapid transfer of saidsecond treating fluid over the surfaces of the textile material and intothe first zone.
 15. In a process for batch treating of textile materialwith a liquid treating agent including a dye liquor, the improvementcomprising: placing the textile material to be treated in an enclosedfirst zone and applying a substantial vacuum in the range of 0 - 10inches of mercury, absolute pressure to the first zone to produce asubstantial negative pressure therein; providing the liquid treatingagent in a second zone; heating the treating agent to a predeterminedtemperature while in the second zone and subjecting the heated treatingagent to a superatmospheric pressure in the second zone; placing thefirst zone in communication with the second zone; and effecting a veryrapid initial transfer of said treating agent from said second zone intosaid first zone wherein said treating agent flows through said textilematerial in an inside-out direction, said transfer taking place at aflow rate of at least about 750 gallons of said treating agent perminute so that said treating agent is uniformly distributed over all orsubstantially all of the surfaces of said textile material substantiallyimmediately after the textile material is first contacted by saidtreating agent and so that said surfaces of said textile material areinitially exposed to or wetted by the treating agent at uniform orsubstantially uniform concentration of said dye liquor; flooding saidfirst zone with the treating agent; isolating the second zone from thefirst zone after the treating agent has flooded the first zone and thenflowing the treating agent from the first zone; flowing the treatingagent removed from the first zone back into the second zone; heating andpressurizing the treating agent in the second zone to a predeterminedtemperature and pressure respectively; evacuating the first zone of theatmosphere therein; and then placing the first zone into communicationwith the second zone to cause recycling of the treating agent from thesecond zone through said textile material into the first zone.
 16. Theprocess defined in claim 1 wherein substantially the entire charge oftreating agent in said second zone is transferred through the textilematerial and into said first zone extremely rapidly.
 17. The processdefined in claim 16 wherein substantially the entire charge of treatingagent in said second zone is transferred through the textile materialand into said first zone is a range of about 0 - 45 seconds.
 18. Theprocess defined in claim 1 wherein the treating agent is recirculatedbetween the second and first zones and through the textile material. 19.The process defined in claim 1 wherein in said initial transfersubstantially the entire charge of treating agent in said second zone istransferred through the textile material in one direction and into saidfirst zone extremely rapidly, and wherein the flow of the treating agentis thereafter reversed to Pass through the textile material in theopposite direction.
 20. The process defined in claim 19 wherein in saidinitial transfer substantially the entire charge of treating agent insaid second zone is transferred through the textile material in said onedirection and into said first zone in a time period of less than about45 seconds.
 21. The process defined in claim 20 wherein the direction offlow is reversed after about 30 seconds.
 22. The process defined inclaim 20 wherein the charge of said treating agent is at least about 800gallons.
 23. The process defined in claim 20 wherein said time period isno greater than about 30 seconds.
 24. The process defined in claim 1wherein the textile material includes a yarn package in the form of yarnwound on a fluid pervious tube, and further wherein the flow of saidtreating agent through said textile material is in a controlleddirection wherein the treating agent is constrained to flow from theinterior of said yarn package outwardly through the yarn.